%0 Journal Article %J Solid State Nuclear Magnetic Resonance %D 2006 %T Solid-state NMR structural studies of the fibril form of a mutant mouse prion peptide PrP89-143(P101L) %A Lim, K. H. %A Nguyen, T. N. %A Damo, S. M. %A Mazur, T. %A Ball, H. L. %A Prusiner, S. B. %A Pines, A. %A Wemmer, D. E. %K identification %X

The peptide fragment 89-143 of the prion protein (carrying a P101L mutation) is biologically active in transgenic mice when in a fibrillar form. Injection of these fibrils into transgenic mice (expressing full length PrP with the P101L mutation) induces a neurodegenerative prion disease (Kaneko et al., J. Mol. Biol. 295 (2000) 997). Here we present solid-state NMR studies of PrP89-143(P101L) fibrils, probing the conformation of residues in the hydrophobic segment 112-124 with chemical shifts. The conformations of glycine residues were analyzed using doubly C-13 = 0 labeled peptides by two-dimensional (2D) double-quantum correlation, and double-quantum filtered dephasing distance measurements. MQ-NMR experiments were carried out to probe the relative alignment of the individual peptides fibrils. These NMR studies indicate that the 112-124 segment adopts an extended beta-sheet conformation, though not in a parallel, in register alignment. There is evidence for conformational variability at Gly 113. DQ correlation experiments provide useful information in regions with conformational heterogeneity. (c) 2005 Elsevier Inc. All rights reserved.

%B Solid State Nuclear Magnetic Resonance %V 29 %P 183-190 %8 Feb %@ 0926-2040 %G English %U ://WOS:000234417500020 %N 1-3 %M WOS:000234417500020 %! Solid-state NMR structural studies of the fibril form of a mutant mouse prion peptide PrP89-143(P101L) %R Doi 10.1016/J.Ssnmr.2005.09.017 %0 Journal Article %J Journal of Magnetic Resonance %D 2002 %T Efficient triple-quantum excitation in modified RIACT MQMAS NMR for I=3/2 nuclei %A Lim, K. H. %A Charpentier, T. %A Pines, A. %K coherence %X

A new approach involving the creation of triple-quantum (TQ) coherences from both TQ and central transitions (CT) is investigated, in order to enhance the efficiency of triple-quantum excitation for I = 3/2 nuclei. The RIACT excitation scheme, a soft pi/2 and hard spin-locking pulse, is shown to induce both adiabatic coherence transfer between CT and TQ coherences and TQ nutation. By combining the RIACT scheme with the presaturation of the satellite transitions, a significant improvement in the TQ excitation can be achieved mainly through enhanced CT polarization via the RIACT mechanism, in particular for nuclei with moderate to large quadrupole coupling constants (greater than or equal to2.0 MHz). There also exists a nontrivial contribution from the TQ transition, which depends on the size of the quadrupole interaction. (C) 2002 Elsevier Science (USA).

%B Journal of Magnetic Resonance %V 154 %P 196-204 %8 Feb %@ 1090-7807 %G English %U ://WOS:000174189300005 %N 2 %M WOS:000174189300005 %! Efficient triple-quantum excitation in modified RIACT MQMAS NMR for I=3/2 nuclei %R Doi 10.1006/Jmre.2001.2471 %0 Journal Article %J Solid State Nuclear Magnetic Resonance %D 2002 %T Investigations of low-amplitude radio frequency pulses at and away from rotary resonance conditions for I=5/2 Nuclei %A Logan, J. W. %A Urban, J. T. %A Walls, J. D. %A Lim, K. H. %A Jerschow, A. %A Pines, A. %K solid-state %X

Additional experimental evidence of rotary resonance effects for multiple-quantum coherence conversion in a spin-5/2 system is presented. Two-dimensional plots of the relative efficiency of MQ excitation and conversion are given as a function of radio frequency (rf) amplitude and pulse width. Data are presented for the excitation of five-quantum coherence (5QC), as well as for 5QC to three-quantum coherence (3QC) conversion, 5QC to 1QC (the central transition coherence) conversion, and 3QC to 1 QC conversion. A two-fold increase in the signal-to-noise ratio is achieved by substituting low amplitude rf pulses in place of hard rf pulses for 5QC excitation and 5QC to 3QC conversion in a mixed multiple-quantum magic angle spinning (MAS) (MMQMAS) experiment. The anisotropic line shape for the low-amplitude rf pulse version of the MMQMAS experiment was observed to be distorted from the MAS line shape. The cause and implications of the distortion are discussed. (C) 2002 Elsevier Science (USA).

%B Solid State Nuclear Magnetic Resonance %V 22 %P 97-109 %8 Sep-Nov %@ 0926-2040 %G English %U ://WOS:000179154400003 %N 2-3 %M WOS:000179154400003 %! Investigations of low-amplitude radio frequency pulses at and away from rotary resonance conditions for I=5/2 Nuclei %R Doi 10.1006/Snmr.2002.0084 %0 Journal Article %J Journal of Magnetic Resonance %D 2002 %T Sensitivity enhancement in multiple-quantum NMR experiments with CPMG detection %A Lim, K. H. %A Nguyen, T. %A Mazur, T. %A Wemmer, D. E. %A Pines, A. %K dynamics %X

We present a modified multiple-quantum (MQ) experiment, which implements the Carr-Purcell-Meiboom-Gill (CPMG) detection scheme in the static MQ NMR experiment proposed by W. S. Warren et al. (1980, J. Chem. Phys. 73, 2084-2099) and exploited further by O. N. Antzutkin and R. Tycko (1999, J. Chem. Phys. 110, 2749-2752). It is demonstrated that a significant enhancement in the sensitivity can be achieved by acquiring echo trains in the MQ experiments for static powder samples. The modified scheme employing the CPMG detection was superior to the original MQ experiment, in particular for the carbonyl carbon with a very large chemical shift anisotropy. (C) 2002 Elsevier Science (USA).

%B Journal of Magnetic Resonance %V 157 %P 160-162 %8 Jul %@ 1090-7807 %G English %U ://WOS:000177742400019 %N 1 %M WOS:000177742400019 %! Sensitivity enhancement in multiple-quantum NMR experiments with CPMG detection %R Doi 10.1006/Jmre.2002.2578 %0 Journal Article %J Journal of Chemical Physics %D 2002 %T Theoretical investigations of I=5/2 quadrupolar spin dynamics in the sudden-passage regime %A Walls, J. D. %A Lim, K. H. %A Logan, J. W. %A Urban, J. T. %A Jerschow, A. %A Pines, A. %K SPECTROSCOPY %X

The theoretical approach utilizing bimodal Floquet theory in the quadrupolar/central-transition interaction frame, presented in an earlier article [J. D. Walls, K. H. Lim, and A. Pines, J. Chem. Phys. 116, 79 (2002)], is extended to describe the more complicated spin dynamics of I=5/2 spin systems. Rotary resonance effects occur when the strength of the radio-frequency irradiation, omega(1), matches the sample spinning speed, omega(r), at the conditions omega(1) = 2/3nomega(r) (n integral). At these conditions, conversions of both triple-quantum and five-quantum coherences to central-quantum coherence are observed. Between rotary resonance conditions [ 2n/3omega(r)<ω(1)<[2(n+1)]/3ω(r)], five-quantum as well as triple-quantum coherences can be created from equilibrium z-magnetization via a nutation mechanism. In addition, effective transfer between five-quantum and triple-quantum coherences also is observed in between rotary resonance conditions. These effects have been investigated theoretically and verified by both numerical calculations and experimental results. (C) 2002 American Institute of Physics.

%B Journal of Chemical Physics %V 117 %P 518-532 %8 Jul 8 %@ 0021-9606 %G English %U ://WOS:000176424800003 %N 2 %M WOS:000176424800003 %! Theoretical investigations of I=5/2 quadrupolar spin dynamics in the sudden-passage regime %R Doi 10.1063/1.1483256 %0 Journal Article %J Journal of Chemical Physics %D 2002 %T Theoretical studies of the spin dynamics of quadrupolar nuclei at rotational resonance conditions %A Walls, J. D. %A Lim, K. H. %A Pines, A. %K solids %X

A theory of the spin dynamics of I=3/2 quadrupolar nuclei in the sudden-passage limit is discussed in relation to the recently observed rotational resonance (RR) effects on the excitation and conversion of triple-quantum coherence in the FASTER multiple-quantum magic-angle spinning (MQMAS) experiments [T. Vosegaard, P. Florian, D. Massiot, and P. J. Grandinetti, J. Chem. Phys. 114, 4618 (2001)]. A novel interaction frame, which combines the quadrupolar interaction with the central transition radio frequency irradiation, is shown to be useful in understanding the complex spin dynamics at and away from RR conditions. Analytical expressions for the Hamiltonian obtained from bimodal Floquet theory are included in order to provide insight into the spin dynamics observed in the FASTER MQMAS experiments. Numerical simulations have been performed and were found to support the theoretical formalism. (C) 2002 American Institute of Physics.

%B Journal of Chemical Physics %V 116 %P 79-90 %8 Jan 1 %@ 0021-9606 %G English %U ://WOS:000172784700010 %N 1 %M WOS:000172784700010 %! Theoretical studies of the spin dynamics of quadrupolar nuclei at rotational resonance conditions %R Doi 10.1063/1.1421613